CN107673405A - A kind of method of recovery chlorine in the technique from titanium dioxide production - Google Patents
A kind of method of recovery chlorine in the technique from titanium dioxide production Download PDFInfo
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- CN107673405A CN107673405A CN201711119430.5A CN201711119430A CN107673405A CN 107673405 A CN107673405 A CN 107673405A CN 201711119430 A CN201711119430 A CN 201711119430A CN 107673405 A CN107673405 A CN 107673405A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G23/00—Compounds of titanium
- C01G23/04—Oxides; Hydroxides
- C01G23/047—Titanium dioxide
- C01G23/07—Producing by vapour phase processes, e.g. halide oxidation
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B7/00—Halogens; Halogen acids
- C01B7/01—Chlorine; Hydrogen chloride
- C01B7/07—Purification ; Separation
- C01B7/0743—Purification ; Separation of gaseous or dissolved chlorine
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Environmental & Geological Engineering (AREA)
- General Life Sciences & Earth Sciences (AREA)
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Abstract
The invention discloses a kind of method of the recovery chlorine in technique from titanium dioxide production, comprise the following steps：Step 1, mixed airflow obtain powder and mixed gas after gas-solid separator separates, and powder is delivered in powder collection device, complete product and collect, mixed gas delivers to CCl4In fluid box；Step 2, CCl4Fluid box is by the CCl after gas washing4Liquid is delivered in the second heat exchanger, and the second heat exchanger is to the CCl after gas washing4Liquid carries out the steps such as degassing that exchange heat.Present invention mainly solves the problems such as the organic efficiency occurred in traditional recovery process is not high, absorbent dosage is larger, caused waste liquid amount is more, purity of chlorine gas feeding is inadequate, by optimizing chlorine recovery system, improve chlorine recovery process, the amount to obtain of chlorine is set significantly to increase, the discharge capacity of chlorine minimizes, and improves the chlorine organic efficiency of chlorine recovery process.
Description
Technical field
The present invention relates to titanium dioxide production technical field, the recovery in more particularly to a kind of technique from titanium dioxide production
The method of chlorine.
Background technology
In the production system of titanium dioxide, pass through TiCl4While vapour phase oxidation process obtains titanium dioxide, it can also produce
Considerable amount of chlorine accessory substance, in order to avoid the waste of resource, chlorine recovery system typically can be all set, however, traditional chlorine
The organic efficiency of gas recovery system is not high, and the dosage of absorbent is larger, and caused waste liquid amount is more, purity of chlorine gas feeding not enough etc. ask
Inscribe, still contain a certain amount of chlorine in the tail gas of discharge, environmental pollution is more serious, therefore, produces the enterprise of titanium dioxide
High pollution enterprise typically is belonged to, is government's environmental protection supervise and examine key monitoring object.
By being investigated and analysed to obtain to the production technology of traditional titanium dioxide production enterprise, cause the master of above mentioned problem
Wanting reason is：Chlorine recovery system is set and the selection of absorbent species is unreasonable, and it is used as absorbent using benzene（Due to
CCl4Belonging to national management and control chemical products, its toxicity is stronger, big to environmental considerations, in view of the jejune situation of traditional handicraft,
In order to obtain qualification of production and not select CCl typically by environmental impact assessment, enterprise4It is used as the absorbent of chlorine）, and chlorine is in benzene
Solubility it is general, less than in CCl4In solubility, still contain considerable amount of chlorine in the tail gas after benzene absorbs, absorb
Tail gas afterwards is after by alkaline solution again gas washing, and externally discharge, in the process, the consumption of alkaline absorption solution is very big,
Waste liquid amount is more, and enterprise can stealthily reduce the usage amount of alkaline absorption solution, thus cause discharge to save production cost
Contain exceeded chlorine in tail gas；Make benzene desorption by way of distillation as benzene absorption chlorine is latter, be derived from chlorine, so
And the solubility due to chlorine in benzene is general, in desorption process is distilled, the escaped quantity of chlorine is less, quick in order to reach
For desorption to reclaim benzene as early as possible, its usual way is to improve vapo(u)rizing temperature to the boiling point of benzene, that is, reaches more than 80 DEG C, with
Make benzene desorption under fluidized state, and then improve the technique effect of desorption rate, such way can make desorption out
Contain considerable amount of benzene in chlorine, thus cause recovery chlorine degree of purity it is relatively low, the usage amount and consumption of benzene are larger.
The content of the invention
The goal of the invention of the present invention is：For above-mentioned problem, there is provided one kind is from titanium dioxide production technique
Recovery chlorine method, by optimizing chlorine recovery system, chlorine recovery process is improved, to solve to go out in traditional recovery process
The problems such as existing organic efficiency is not high, the dosage of absorbent is larger, caused waste liquid amount is more, purity of chlorine gas feeding is inadequate.
The technical solution adopted by the present invention is as follows：A kind of method of recovery chlorine in the technique from titanium dioxide production, its
It is characterised by, comprises the following steps：
Step 1, O2With TiCl4Mixed airflow is obtained after hybrid reaction in tubular type high-temperature reactor, mixed airflow is through gas-solid point
Powder and mixed gas are obtained after being separated from device, powder is sent to powder collection device by the powder output end of gas-solid separator
It is interior, complete product and collect, mixed gas is sent to CCl by the gas output end of gas-solid separator4Gas washing is carried out in fluid box,
To reclaim the chlorine in mixed gas, the mixed gas after gas washing passes through CCl4The gas output end of fluid box delivers to vent gas treatment
Unit, after tail gas treating unit is handled the mixed gas after gas washing and reaches discharge standard, directly externally discharge；
Step 2, CCl4Fluid box is by the CCl after gas washing4Liquid is delivered in the second heat exchanger by its fluid output port, and second changes
Hot device is to the CCl after gas washing4Liquid carries out heat exchange heating, then delivers to caused gas and gas washing is carried out in benzene respiratory box, remains
Remaining CCl4Liquid is sent into CCl after cooling4It is continuing with liquid recovery tank；
Step 3, benzene respiratory box carry out gas washing to the gas that the second heat exchanger is sent below 50 DEG C, and the gas after gas washing is directly sent
To chlorine recycling can, the benzene after gas washing, which is sent in distiller, to be distilled；
Step 4, distiller distill to the benzene after gas washing, obtain retort gas and distillating liquid, retort gas it is condensed into
CCl is sent into after liquid4It is continuing with fluid box, distillating liquid is sent into benzene respiratory box and is continuing with after cooling.
Further, in step 3, heat exchanger makes the CCl after gas washing4The temperature of liquid reaches 60-75 DEG C.
Further, in step 5, vapo(u)rizing temperature is controlled at 70-76 DEG C.
In the present invention, in order that the tail gas of discharge can reach discharge standard, tail gas treating unit includes NaOH solution
Case, the input connection CCl of NaOH solution case4The gas output end of fluid box, NaOH solution case are used to carry out gas washing to gas,
After gas after gas washing reaches discharge standard, directly externally discharge.
Further, in order to improve the gas-solid separating effect of gas-solid separator, the content of powder in mixed gas is reduced, and then
Pollution level of the powder to absorbent is reduced, the input of gas-solid separator is connected by First Heat Exchanger and tubular type high-temperature reactor
Connect, to reduce the temperature of mixed airflow using First Heat Exchanger.
Further, the coolant output end of First Heat Exchanger connects the coolant input of the second heat exchanger, with fully profit
With the heat of the coolant of First Heat Exchanger.In above-mentioned, the mixed air-flow that deteriorates is cooled using First Heat Exchanger, Jin Erti
The gas-solid separating effect of high gas-solid separator, powder content is few in obtained mixed gas, can be neglected, in the first heat exchange
In device, heat possessed by the cooling water after heat exchange can be as the thermal source of the second heat exchanger, for CCl4Degassing process
Process, heat has been obtained abundant use, avoid the waste of the energy.
In summary, by adopting the above-described technical solution, the beneficial effects of the invention are as follows：It is provided by the invention it is a kind of from
The method of recovery chlorine in titanium dioxide production technique, mainly solves the organic efficiency occurred in traditional recovery process not
High, the problems such as dosage of absorbent is larger, caused waste liquid amount is more, purity of chlorine gas feeding is inadequate, by optimizing chlorine recovery system,
Chlorine recovery process is improved, the amount to obtain of chlorine is significantly increased, the discharge capacity of chlorine minimizes, and improves chlorine recovery work
The chlorine organic efficiency of skill.
Brief description of the drawings
Fig. 1 is the system structure diagram of the recovery chlorine in a kind of technique from titanium dioxide production of the present invention.
Marked in figure：1 is gas-solid separator, and 2 be powder collection device, and 3 be CCl4Fluid box, 4 be chlorine recycling can, 5
It is benzene respiratory box for the second heat exchanger, 6,7 be distiller, and 8 be CCl4Liquid tank, 9 be First Heat Exchanger, and 10 be that tubular type high temperature is anti-
Answer device.
Embodiment
Below in conjunction with the accompanying drawings, the present invention is described in detail.
In order to make the purpose , technical scheme and advantage of the present invention be clearer, it is right below in conjunction with drawings and Examples
The present invention is further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, and
It is not used in the restriction present invention.
As shown in figure 1, a kind of system of the recovery chlorine in technique from titanium dioxide production, including gas-solid separator 1, gas
The powder output end connection powder collection device 2 of solid separator 1, the gas output end connection CCl of gas-solid separator 14Fluid box 3
An input, CCl4The fluid output port connection degassing recovery unit of fluid box 3, CCl4The gas output end of fluid box 3 connects
Tail gas treating unit is connect, degassing recovery unit is used for CCl4Liquid is de-gassed processing, the gas output for the recovery unit that deaerates
End connection chlorine recycling can 4, the fluid output port connection CCl for the recovery unit that deaerates4Fluid box 3.
In the present invention, CCl is utilized4Liquid overcomes conventional art to CCl4Using ground prejudice, chlorine is in CCl4In have
Solubility well, CCl4Liquid can largely absorb the chlorine in mixing mixed gas, and then make the chlorine content in tail gas
It is greatly reduced, tail gas is being that alkali lye consumption amount is few and waste liquid yield is few, enters without enterprise by tail gas treating unit processing
Deliberately go to reduce the usage amount of alkali lye to reduce production cost, the setting containing unconventional gas recovery unit, eliminate CCl4
Using when easily cause the misgivings of environmental pollution, realize CCl4Reuse, solve the recovery occurred in traditional recovery process
The problems such as efficiency is not high, the dosage of absorbent is larger, caused waste liquid amount is more, purity of chlorine gas feeding is inadequate.
In order to preferably implement the present invention, degassing recovery unit includes being used for the second heat exchanger 5 for heating up to supplied materials,
The input connection CCl of second heat exchanger 54The fluid output port of fluid box 3, an output end of the second heat exchanger 5 connect
Meet chlorine recycling can 4, another output end connection CCl of the second heat exchanger 54Fluid box 3.Helped by the second heat exchanger 5
CCl4There is ground tubular structure can improve CCl for degassing, the second heat exchanger 54Heat exchange efficiency, promote it rapidly to discharge chlorine
Gas, without being heated to CCl4Boiling point on, thereby reduce CCl4Escaped quantity, be effectively improved chlorine
Degree of purity, meanwhile, the present invention is not required for CCl4All degassings, it is remaining as long as wherein 80% chlorine can be removed
CCl4CCl is delivered to by circulation line4It is continuing with fluid box 3, and then improves CCl4Absorbent utilizes power, nothing
Substantial amounts of CCl need to be used4To reclaim chlorine.
Further, ground CCl is escaped in order to reclaim4Liquid, improves the degree of purity of chlorine, and one of the second heat exchanger 5 is defeated
Go out end and chlorine recycling can 4 is connected by benzene respiratory box 6.CCl is absorbed using benzene respiratory box 64Liquid, improve the pure of chlorine
Degree, reduces CCl4The consumption of liquid, due to CCl4Escaped quantity it is less, therefore benzene respiratory box 6 is separated without the short time
Recovery, treat the CCl that benzene respiratory box 6 absorbs4After reaching finite concentration, separated to it, greatly improving chlorine degree of purity
While, effectively reduce CCl4Loss, it is therefore prevented that CCl4The problem of leakage pollution environment.
Further, in order to reclaim CCl from benzene respiratory box 64, and benzene respiratory box 6 is possessed absorption CCl again4Work(
Can, 6 one output end connection distillers 7 of benzene respiratory box, an input of the output end connection benzene respiratory box 6 of distiller 7
End, another output end connection CCl of distiller 74Fluid box 3.The benzene liquid in benzene respiratory box 6 is carried out by distiller 7
Distillation, because the boiling point of benzene is higher than CCl4Boiling point, set vapo(u)rizing temperature in CCl4Boiling point near, in heating process, benzene
The chlorine and a small amount of CCl that liquid escapes first4, the portion gas is passed directly into benzene respiratory box 6 to handle, and temperature to be distilled reaches 60
More than DEG C, mainly with CCl in effusion ground gas4Based on, obtain the CCl dissolved with fraction chlorine after the portion gas is condensed4Liquid
Body, the partially liq is passed directly into CCl4Reused in fluid box 3, treat that the gas escaped quantity in benzene liquid significantly reduces
And when less, stop distillation, directly by being continuing with benzene respiratory box 6 after remaining benzene liquid is cooled down.Whole process benzene, CCl4
No consumption equal with chlorine and discharge, and then while zero-emission is reached, effectively reduce the consumption of raw material.
Further, in order to CCl is better achieved4Recycling, an output end of the second heat exchanger 5 passes through CCl4
Liquid tank 8 connects CCl4Fluid box 3, CCl4One input of liquid tank 8 connects the second heat exchanger 5, and its another input connects
Connect distiller 7, CCl4The output end connection CCl of liquid tank 84Fluid box 3.
Further, in order to improve the gas-solid separating effect of gas-solid separator 1, the content of powder in mixed gas is reduced,
And then pollution level of the powder to absorbent is reduced, the input of gas-solid separator 1 is anti-by First Heat Exchanger 9 and tubular type high temperature
Device 10 is answered to connect, the coolant output end of First Heat Exchanger 9 connects the coolant input of the second heat exchanger 5.
In above-mentioned, mixed airflow is cooled using First Heat Exchanger 9, and then improves the gas-solid of gas-solid separator 1
Separating effect, powder content is few in obtained mixed gas, can be neglected, cold after heat exchange in First Heat Exchanger 9
But heat possessed by water, can be as the thermal source of the second heat exchanger 5, for CCl4Degassing process process, thus make heat
Abundant use has been obtained, has avoided the waste of the energy.
In the present invention, in order that the tail gas of discharge can reach discharge standard, tail gas treating unit includes NaOH solution
Case, the input connection CCl of NaOH solution case4The gas output end of fluid box, NaOH solution case are used to carry out gas washing to gas,
After gas after gas washing reaches discharge standard, directly externally discharge.
Present invention additionally comprises a kind of method of the recovery chlorine in technique from titanium dioxide production, comprise the following steps：
Step 1, O2With TiCl4Mixed airflow is obtained after hybrid reaction in tubular type high-temperature reactor 10, mixed airflow is through gas-solid
Separator 1 obtains powder and mixed gas after separating, powder is sent to powder by the powder output end of gas-solid separator 1 and collected
In device 2, complete product and collect, mixed gas is sent to CCl by the gas output end of gas-solid separator 14Enter in fluid box 3
Row gas washing, to reclaim the chlorine in mixed gas, the mixed gas after gas washing passes through CCl4The gas output end of fluid box 3 is delivered to
Tail gas treating unit, it is directly right after tail gas treating unit is handled the mixed gas after gas washing and reaches discharge standard
Outer discharge；
Step 2, CCl4Fluid box 3 is by the CCl after gas washing4Liquid is delivered in the second heat exchanger 5 by its fluid output port, and second
Heat exchanger 5 is to the CCl after gas washing4Liquid carries out heat exchange heating, makes the CCl after gas washing4The temperature of liquid reaches 60-75 DEG C（Specifically
Temperature is adjusted according to actual conditions）, then caused gas is delivered to gas washing, remaining CCl is carried out in benzene respiratory box 64Liquid
Body is sent into CCl after cooling4It is continuing with fluid box 3；
Step 3, benzene respiratory box 6 carry out gas washing to the gas that the second heat exchanger 5 is sent below 50 DEG C, and the gas after gas washing is direct
Deliver in chlorine recycling can 4, the benzene after gas washing, which is sent in distiller 7, to be distilled；
Step 4, distiller 7 are distilled to the benzene after gas washing, and vapo(u)rizing temperature is controlled at 70-76 DEG C（Actual temp is according to reality
Situation is adjusted）, obtain retort gas and distillating liquid, retort gas is condensed into being sent into CCl after liquid4In fluid box 3 after
Continuous to use, distillating liquid is sent into benzene respiratory box 6 and is continuing with after cooling.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all essences in the present invention
All any modification, equivalent and improvement made within refreshing and principle etc., should be included in the scope of the protection.
Claims (6)
1. the method for the recovery chlorine in a kind of technique from titanium dioxide production, it is characterised in that comprise the following steps：
Step 1, O2With TiCl4Mixed airflow is obtained after hybrid reaction in tubular type high-temperature reactor, mixed airflow is through gas solid separation
Powder and mixed gas are obtained after device separation, powder is sent to powder collection device by the powder output end of gas-solid separator
It is interior, complete product and collect, mixed gas is sent to CCl by the gas output end of gas-solid separator4Gas washing is carried out in fluid box,
To reclaim the chlorine in mixed gas, the mixed gas after gas washing passes through CCl4The gas output end of fluid box delivers to vent gas treatment
Unit, after tail gas treating unit is handled the mixed gas after gas washing and reaches discharge standard, directly externally discharge；
Step 2, CCl4Fluid box is by the CCl after gas washing4Liquid is delivered in the second heat exchanger by its fluid output port, and second changes
Hot device is to the CCl after gas washing4Liquid carries out heat exchange heating, then delivers to caused gas and gas washing is carried out in benzene respiratory box, remains
Remaining CCl4Liquid is sent into CCl after cooling4It is continuing with liquid recovery tank；
Step 3, benzene respiratory box carry out gas washing to the gas that the second heat exchanger is sent below 50 DEG C, and the gas after gas washing is directly sent
To chlorine recycling can, the benzene after gas washing, which is sent in distiller, to be distilled；
Step 4, distiller distill to the benzene after gas washing, obtain retort gas and distillating liquid, retort gas it is condensed into
CCl is sent into after liquid4It is continuing with fluid box, distillating liquid is sent into benzene respiratory box and is continuing with after cooling.
2. the method for the recovery chlorine in a kind of technique from titanium dioxide production as claimed in claim 1, it is characterised in that step
In rapid 3, heat exchanger makes the CCl after gas washing4The temperature of liquid reaches 60-75 DEG C.
3. the method for the recovery chlorine in a kind of technique from titanium dioxide production as claimed in claim 1, it is characterised in that step
In rapid 5, vapo(u)rizing temperature is controlled at 70-76 DEG C.
4. the method for the recovery chlorine in a kind of technique from titanium dioxide production as claimed in claim 1, it is characterised in that tail
Gas disposal unit includes NaOH solution case, the input connection CCl of NaOH solution case4The gas output end of fluid box, NaOH are molten
Liquid case is used to carry out gas gas washing, after the gas after gas washing reaches discharge standard, directly externally discharge.
5. the method for the recovery chlorine in a kind of technique from titanium dioxide production as claimed in claim 1, it is characterised in that gas
The input of solid separator is connected by First Heat Exchanger with tubular type high-temperature reactor, to reduce mixing using First Heat Exchanger
The temperature of air-flow.
6. the method for the recovery chlorine in a kind of technique from titanium dioxide production as claimed in claim 5, it is characterised in that the
The coolant output end of one heat exchanger connects the coolant input of the second heat exchanger, to make full use of the cooling of First Heat Exchanger
The heat of liquid.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201711119430.5A CN107673405A (en) | 2017-11-14 | 2017-11-14 | A kind of method of recovery chlorine in the technique from titanium dioxide production |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711119430.5A CN107673405A (en) | 2017-11-14 | 2017-11-14 | A kind of method of recovery chlorine in the technique from titanium dioxide production |
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Application publication date: 20180209 |